EP0141312A1 - Method for the preparation of solid cyanuric chloride - Google Patents
Method for the preparation of solid cyanuric chloride Download PDFInfo
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- EP0141312A1 EP0141312A1 EP84112227A EP84112227A EP0141312A1 EP 0141312 A1 EP0141312 A1 EP 0141312A1 EP 84112227 A EP84112227 A EP 84112227A EP 84112227 A EP84112227 A EP 84112227A EP 0141312 A1 EP0141312 A1 EP 0141312A1
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- European Patent Office
- Prior art keywords
- cyanuric chloride
- cold air
- vapor
- separation chamber
- solid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000007787 solid Substances 0.000 title claims abstract description 12
- 239000007789 gas Substances 0.000 claims abstract description 10
- 238000005829 trimerization reaction Methods 0.000 claims abstract description 7
- QPJDMGCKMHUXFD-UHFFFAOYSA-N cyanogen chloride Chemical compound ClC#N QPJDMGCKMHUXFD-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000011084 recovery Methods 0.000 claims abstract description 5
- 230000008021 deposition Effects 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims description 20
- 239000010419 fine particle Substances 0.000 abstract description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 4
- 229910052801 chlorine Inorganic materials 0.000 description 4
- 239000000460 chlorine Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- MXWJVTOOROXGIU-UHFFFAOYSA-N atrazine Chemical compound CCNC1=NC(Cl)=NC(NC(C)C)=N1 MXWJVTOOROXGIU-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 239000000110 cooling liquid Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 239000011541 reaction mixture Substances 0.000 description 2
- QMNWYGTWTXOQTP-UHFFFAOYSA-N 1h-triazin-6-one Chemical class O=C1C=CN=NN1 QMNWYGTWTXOQTP-UHFFFAOYSA-N 0.000 description 1
- MIEBPIZYROEIGP-UHFFFAOYSA-N CC(C)CCN1CC1 Chemical compound CC(C)CCN1CC1 MIEBPIZYROEIGP-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000002028 premature Effects 0.000 description 1
- 239000011814 protection agent Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
- C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
- C07D251/12—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
- C07D251/26—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hetero atoms directly attached to ring carbon atoms
- C07D251/28—Only halogen atoms, e.g. cyanuric chloride
Definitions
- the present invention relates to a process for the production of solid cyanuric chloride in finely divided form.
- Cyanuric chloride which is of considerable technical importance as an intermediate for the production of dyes, crop protection agents, pharmaceuticals and textile and rubber auxiliaries, is obtained after the catalytic trimerization of cyanogen chloride in gaseous form, together with unreacted cyanogen chloride and chlorine. This gas mixture was usually passed into separation chambers and the cyanuric chloride was deposited on the cooled walls.
- a disadvantage of this type of desublimation is that the cyanuric chloride in the form of coarse crystals settles on the walls and discharge devices and thus has a negative effect on the heat transfer. Regular tapping of the crystals from the walls leads to a brief improvement in the heat transfer, but this method is by no means satisfactory because of the increasing mechanical damage and noise pollution, not to mention the poor quality of the product obtained in this way.
- DE-AS 28 43 381 and DE-AS 28 43 382 describe processes for the recovery of liquid or solid cyanuric chloride, according to which the reaction mixture obtained after the trimerization of cyanuric chloride is introduced into and through an apparatus combination consisting of stripping column and condenser Temperature control and admixing of inert gas (to prevent total condensation) at the outlet of the condenser partially condenses the cyanuric chloride in the column, while the gaseous fraction that emerges at the top of the column is desublimated in the usual separation chambers.
- the disadvantage of this method is the complex apparatus combination, which causes high investment and operating costs.
- the present invention is therefore based on the object of developing a process for obtaining solid cyanuric chloride which does not have the disadvantages of the prior art described and which provides a cyanuric chloride without great technical outlay and which gives satisfactory results with regard to the particle size distribution and purity of the product.
- cyanuric chloride vapor is introduced simultaneously with a separately supplied stream of cold air through obliquely upward feed lines into a separation chamber such that there is an intensive mixing of the cyanuric chloride vapor with the cold air after the two currents meet exhaust gases free of cyanuric chloride in the upper part of the separation chamber and the solid cyanuric chloride is discharged from the lower part of the separation chamber.
- the cyanuric chloride vapor which is still numerous impurities such.
- B. contains chlorine cyanide or chlorine, after leaving the trimerization reactor passed into the separation chamber. Since no partial pressure-reducing gas is added, the line between the reactor and the separation chamber must be thermally insulated in order to prevent premature condensation of the cyanuric chloride, which can lead to undesired blockages.
- the gaseous reaction mixture should expediently have a temperature between 250 and 300 ° C. before entering the separation chamber, so that a good quenching effect by the cold air is ensured.
- the hot cyanuric chloride vapors are preferably blown into the lower part of the separation chamber together with separately supplied cold air through an obliquely upward feed line, the cold air preferably having a temperature of 0 to 60 ° C., in particular 10 to 25 ° C.
- the feed line should expediently have an angle of 10 to 80 °, preferably 30 to 50 °, with respect to the horizontal, so that there is good air circulation within the separation chamber, which is also associated with good heat exchange. In this way, the undesired deposition of coarse crystals on the walls and discharge devices is prevented and the deposition process is also considerably accelerated.
- cold air to the separators to the cyanuric chloride vapor in amounts of 20 to 150 kg, preferably 50 to 75 kg, per 100 kg of cyanuric chloride vapor.
- An arrangement of several, in particular four or more, cold air nozzles, which are arranged obliquely and tangentially to the cyanuric chloride flow relative to the cyanuric chloride feed, has proven to be particularly advantageous.
- These rapidly emerging cold air flows have an ejector effect and entrain room air in proportion to their mass and the square of their speed.
- the amount of room air sucked in is generally 10 3 times the amount of ejector air blown in.
- the intensive mixing of this large amount of gas leads to a quenching effect in seconds, which allows the cyanuric chloride to condense out in a particularly fine-particle form.
- the cyanuric chloride then separates out very quickly in the air stream and is thereby obtained in a particularly fine-particle form (preferably at most 3 to 4% of the particles have a grain size> 60 ⁇ m).
- the product is discharged in the lower part of the separation chamber, while the practically cyanuric chloride-free exhaust gases are extracted in the upper part of the chamber.
- the cyanuric chloride produced according to the invention surprisingly also already has a very high degree of purity (cyanuric chloride content> 99.5%, hydroxytriazines (0.5%, polytriazines ⁇ 0.1%) and can therefore be processed directly in most cases without further cleaning operations
- cyanuric chloride according to the invention for example, atrazine is obtained in a yield of 99%, which with cyanuric chloride obtained according to the prior art was not possible directly.
- the extremely high grain size also leads to a strong increase in reactivity. The reaction time for the production of atrazine is considerably reduced.
- the drawing shows schematically the recovery of solid cyanuric chloride from the reaction gas mixture obtained during the trimerization of the cyanogen chloride.
- the cyanuric chloride vapor is fed through line (1) to the separation chamber (5) in the lower part.
- the line (1) is directed obliquely upwards at the entry into the chamber (5).
- Cold air is introduced through the nozzles (2).
- the solid is discharged via line (3), while the exhaust gases are drawn off via line (4) at the upper part of the separation chamber (5).
- the feed line (1) After leaving the trimerization reactor, the resulting cyanuric chloride vapor, which still contains impurities such as e.g. B. contains chlorine or chlorine, in an amount of 250 kg / h in the lower part of the separation chamber (5) according to the drawing, the feed line (1) has an angle of 45 ° to the horizontal.
- 135 kg / h of cold air at a temperature of 25 ° C are passed through several nozzles (2) into the separating chamber (5), thus causing the deposition of the cyanuric chloride. While the cold air is extracted together with the residual gases at the upper part of the separation chamber, the fine-particle, solid cyanuric chloride accumulates at the bottom of the separation chamber, where it is discharged.
- the resulting cyanuric chloride has the following particle size distribution:
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Treating Waste Gases (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
Es wird ein Verfahren zur Gewinnung von festem Cyanurchlorid aus dem bei der Trimerisierung von Chlorcyan anfallenden Cyanurchloriddampf durch Abscheidung in einer Abscheidekammer beschrieben, das dadurch gekennzeichnet ist, daß man den Cyanurchloriddampf getrennt von kalter Luft durch eine schräg nach oben gerichtete Zuleitung derart in die Abscheidekammer einbläst, daß eine intensive Durchmischung des Cyanurchloriddampfes mit der Kaltluft und mitgerissenen Raumluft erfolgt, die cyanurchloridfreien Abgase im oberen Teil der Abscheidekammer abzieht und das feste Cyanurchlorid aus dem unteren Teil der Abscheidekammer austrägt. Nach diesem Verfahren wird ein feinteiliges Cyanurchlorid erhalten, das auch bereits einen sehr hohen Reinheitsgrad aufweist.A process for the recovery of solid cyanuric chloride from the cyanuric chloride vapor obtained in the trimerization of cyanogen chloride by deposition in a separating chamber is described, which is characterized in that the cyanuric chloride vapor is blown into the separating chamber separately from cold air by an obliquely upward feed line that an intensive mixing of the cyanuric chloride vapor with the cold air and entrained room air takes place, the cyanuric chloride-free exhaust gases are drawn off in the upper part of the separating chamber and the solid cyanuric chloride is discharged from the lower part of the separating chamber. A fine-particle cyanuric chloride is obtained by this process, which already has a very high degree of purity.
Description
Die vorliegende Erfindung betrifft ein Verfahren zur Gewinnung von festem Cyanurchlorid in feinverteilter Form.The present invention relates to a process for the production of solid cyanuric chloride in finely divided form.
Cyanurchlorid, welches als Zwischenprodukt für die Herstellung von Farbstoffen, Pflanzenschutzmitteln, Pharmazeutika sowie Textil- und Kautschukhilfsmitteln erhebliche technische Bedeutung besitzt, fällt nach der katalytischen Trimerisierung von Chlorcyan in gasförmiger Form an, zusammen mit nicht umgesetztem Chlorcyan und Chlor. Dieses Gasgemisch wurde üblicherweise in Abscheidekammern geleitet und das Cyanurchlorid an den gekühlten Wänden abgeschieden. Nachteilig bei dieser Art der Desublimation ist, daß sich das Cyanurchlorid in Form grober Kristalle an den Wänden und Austragsvorrichtungen absetzt und somit den Wärmeübergang negativ beeinflußt. Regelmäßiges Abklopfen der Kristalle von den Wänden führt zwar zu einer kurzzeitigen Verbesserung des Wärmeüberganges, doch ist diese Methode wegen der zunehmenden mechanischen Beschädigung und der Lärmbelästigung keineswegs befriedigend, ganz abgesehen von der schlechten Qualität des auf diese Weise erhaltenen Produkts.Cyanuric chloride, which is of considerable technical importance as an intermediate for the production of dyes, crop protection agents, pharmaceuticals and textile and rubber auxiliaries, is obtained after the catalytic trimerization of cyanogen chloride in gaseous form, together with unreacted cyanogen chloride and chlorine. This gas mixture was usually passed into separation chambers and the cyanuric chloride was deposited on the cooled walls. A disadvantage of this type of desublimation is that the cyanuric chloride in the form of coarse crystals settles on the walls and discharge devices and thus has a negative effect on the heat transfer. Regular tapping of the crystals from the walls leads to a brief improvement in the heat transfer, but this method is by no means satisfactory because of the increasing mechanical damage and noise pollution, not to mention the poor quality of the product obtained in this way.
Gemäß der DE-AS 12 66 308 versuchte man dieses Problem dadurch zu umgehen, daß man Cyanurchlorid zusammen mit einer leicht verdampfenden inerten Kühlflüssigkeit wie z. B. Chloroform versprüht. Man erhält auf diese Weise zwar ein feinverteiltes Cyanurchlorid, doch ist die Rückgewinnung der Kühlflüssigkeit ziemlich aufwendig. Darüberhinaus kann es sehr leicht zu Verstopfungen der Düse kommen.According to DE-AS 12 66 308 an attempt was made to avoid this problem by adding cyanuric chloride together with a readily evaporating inert cooling liquid such as. B. sprayed chloroform. A finely divided cyanuric chloride is obtained in this way, but the recovery of the cooling liquid is rather complex. In addition, the nozzle can become clogged very easily.
Schließlich werden in der DE-AS 28 43 381 und der DE-AS 28 43 382 Verfahren zur Gewinnung von flüssigem oder festem Cyanurchlorid beschrieben, nach denen man das nach der Trimerisierung von Cyanurchlorid anfallende Reaktionsgemisch in eine Apparatekombination bestehend aus Abtriebskolonne und Kondensator einleitet und durch Temperaturregelung und Zumischen von Inertgas (zur Verhinderung von Totalkondensation) am Austritt des Kondensators das Cyanurchlorid in der Kolonne teilweise kondensiert, während der gasförmige Anteil, der am Kolonnenkopf austritt, in den üblichen Abscheidekammern desublimiert wird. Nachteilig bei dieser Methode ist die aufwendige Apparatekombination, die hohe Investitions- und Betriebskosten verursacht.Finally, DE-AS 28 43 381 and DE-AS 28 43 382 describe processes for the recovery of liquid or solid cyanuric chloride, according to which the reaction mixture obtained after the trimerization of cyanuric chloride is introduced into and through an apparatus combination consisting of stripping column and condenser Temperature control and admixing of inert gas (to prevent total condensation) at the outlet of the condenser partially condenses the cyanuric chloride in the column, while the gaseous fraction that emerges at the top of the column is desublimated in the usual separation chambers. The disadvantage of this method is the complex apparatus combination, which causes high investment and operating costs.
Der vorliegenden Erfindung liegt daher die Aufgabe zugrunde, ein Verfahren zur Gewinnung von festem Cyanurchlorid zu entwickeln, welches die geschilderten Nachteile des Standes der Technik nicht aufweist und ohne großen technischen Aufwand ein Cyanurchlorid bereitstellt, das hinsichtlich der Kornverteilung und Reinheit des Produktes befriedigende Ergebnisse liefert.The present invention is therefore based on the object of developing a process for obtaining solid cyanuric chloride which does not have the disadvantages of the prior art described and which provides a cyanuric chloride without great technical outlay and which gives satisfactory results with regard to the particle size distribution and purity of the product.
Diese Aufgabe wird erfindungsgemäß dadurch gelöst, daß man den Cyanurchloriddampf gleichzeitig mit einem getrennt zugeführten Strom kalter Luft durch schräg nach oben gerichtete Zuleitungen derart in eine Abscheidekammer einleitet, daß es nach dem Zusammentreffen beider Ströme zu einer intensiven Durchmischung des Cyanurchloriddampfes mit der Kaltluft kommt, die cyanurchloridfreien Abgase im oberen Teil der Abscheidekammer abzieht und das feste Cyanurchlorid aus dem unteren Teil der Abscheidekammer austrägt.This object is achieved in that the cyanuric chloride vapor is introduced simultaneously with a separately supplied stream of cold air through obliquely upward feed lines into a separation chamber such that there is an intensive mixing of the cyanuric chloride vapor with the cold air after the two currents meet exhaust gases free of cyanuric chloride in the upper part of the separation chamber and the solid cyanuric chloride is discharged from the lower part of the separation chamber.
Nach diesem Verfahren wird überraschenderweise ein äußerst feinteiliges und gleichzeitig sehr reines Cyanurchlorid erhalten, wodurch sich aufwendige Apparaturen für zusätzliche Reinigungsschritte erübrigen.This process surprisingly gives an extremely finely divided and at the same time very pure cyanuric chloride, making complex apparatuses unnecessary for additional cleaning steps.
Gemäß der Erfindung wird der Cyanurchloriddampf, der noch zahlreiche Verunreinigungen wie z. B. Chlorcyan oder Chlor enthält, nach dem Austritt aus dem Trimerisierungsreaktor in die Abscheidekammer geleitet. Da kein partialdruckerniedrigendes Gas zugesetzt wird, muß die Leitung zwischen Reaktor und Abscheidekammer wärmeisoliert werden, um eine vorzeitige Kondensation des Cyanurchlorids zu verhindern, die zu unerwünschten Verstopfungen führen kann.According to the invention, the cyanuric chloride vapor, which is still numerous impurities such. B. contains chlorine cyanide or chlorine, after leaving the trimerization reactor passed into the separation chamber. Since no partial pressure-reducing gas is added, the line between the reactor and the separation chamber must be thermally insulated in order to prevent premature condensation of the cyanuric chloride, which can lead to undesired blockages.
Das gasförmige Reaktionsgemisch sollte vor dem Eintritt in die Abscheidekammer zweckmäßigerweise eine Temperatur zwischen 250 und 300°C aufweisen, damit ein guter Abschreckeffekt durch die Kaltluft gewährleistet ist. Die heißen Cyanurchloriddämpfe werden durch eine schräg nach oben gerichtete Zuleitung vorzugsweise in den unteren Teil der Abscheidekammer zusammen mit getrennt zugeführter kalter Luft eingeblasen, wobei die Kaltluft vorzugsweise eine Temperatur von 0 bis 60°C, insbesondere von 10 bis 25°C besitzt. Die Zuleitung sollte gegenüber der Horizontalen zweckmäßigerweise einen Winkel von 10 bis 80°, vorzugsweise von 30 bis 50° aufweisen, damit es zu einer guten Luftumwälzung innerhalb der Abscheidekammer kommt, womit auch ein guter Wärmeaustausch verbunden ist. Auf diese Weise wird die unerwünschte Abscheidung grober Kristalle an den Wänden und Austragsvorrichtungen verhindert und außerdem der Abscheidevorgang wesentlich beschleunigt.The gaseous reaction mixture should expediently have a temperature between 250 and 300 ° C. before entering the separation chamber, so that a good quenching effect by the cold air is ensured. The hot cyanuric chloride vapors are preferably blown into the lower part of the separation chamber together with separately supplied cold air through an obliquely upward feed line, the cold air preferably having a temperature of 0 to 60 ° C., in particular 10 to 25 ° C. The feed line should expediently have an angle of 10 to 80 °, preferably 30 to 50 °, with respect to the horizontal, so that there is good air circulation within the separation chamber, which is also associated with good heat exchange. In this way, the undesired deposition of coarse crystals on the walls and discharge devices is prevented and the deposition process is also considerably accelerated.
Zur Erzielung des erfindungsgemäßen Effektes ist es vorteilhaft, dem Cyanurchloriddampf Kaltluft in Mengen von 20 bis 150 kg, vorzugsweise 50 bis 75 kg pro 100 kg Cyanurchloriddampf den Abscheidern zuzumischen. Als besonders vorteilhaft hat sich eine Anordnung von mehreren, insbesondere vier oder mehr Kaltluft-Düsen erwiesen, welche gegenüber der Cyanurchloridzuleitung schräg und tangential zum Cyanurchlorid-Strom angeordnet sind. Diese schnell austretenden Kaltluftströme haben eine Ejektorwirkung und reißen proportional zu ihrer Masse und dem Quadrat ihrer Geschwindigkeit Raumluft mit. Die angesaugte Raumluftmenge beträgt im allgemeinen das 103-fache der eingeblasenen Ejektorluftmenge. Die intensive Durchmischung dieser großen Gasmenge führt in Sekunden zu einem Abschreckeffekt, der das Cyanurchlorid in besonders feinteiliger Form auskondensieren läßt. Das Cyanurchlorid scheidet sich dann sehr rasch im Luftstrom ab und fällt hierbei in einer besonders feinteiligen Form (vorzugsweise besitzen höchstens 3 bis 4 % der Teilchen eine Korngröße >60 µm) an. Das Produkt wird im unteren Teil der Abscheidekammer ausgetragen, während die praktisch cyanurchloridfreien Abgase im oberen Teil der Kammer abgezogen werden.To achieve the effect according to the invention, it is advantageous to add cold air to the separators to the cyanuric chloride vapor in amounts of 20 to 150 kg, preferably 50 to 75 kg, per 100 kg of cyanuric chloride vapor. An arrangement of several, in particular four or more, cold air nozzles, which are arranged obliquely and tangentially to the cyanuric chloride flow relative to the cyanuric chloride feed, has proven to be particularly advantageous. These rapidly emerging cold air flows have an ejector effect and entrain room air in proportion to their mass and the square of their speed. The amount of room air sucked in is generally 10 3 times the amount of ejector air blown in. The intensive mixing of this large amount of gas leads to a quenching effect in seconds, which allows the cyanuric chloride to condense out in a particularly fine-particle form. The cyanuric chloride then separates out very quickly in the air stream and is thereby obtained in a particularly fine-particle form (preferably at most 3 to 4% of the particles have a grain size> 60 μm). The product is discharged in the lower part of the separation chamber, while the practically cyanuric chloride-free exhaust gases are extracted in the upper part of the chamber.
Neben dieser Feinteiligkeit besitzt das erfindungsgemäß hergestellte Cyanurchlorid überraschenderweise bereits auch einen sehr hohen Reinheitsgrad (Cyanurchloridgehalt >99,5 %, Hydroxytriazine (0,5 %, Polytriazine <0,1 %) und kann deshalb in den meisten Fällen ohne weitere Reinigungsoperationen direkt weiterverarbeitet werden. Mit dem erfindungsgemäßen Cyanurchlorid wird z. B. Atrazin in einer Ausbeute von 99 % erhalten, was mit nach dem Stand der Technik erhaltenem Cyanurchlorid direkt nicht möglich war. Die extrem hohe Kornfeinheit führt außerdem zu einer starken Erhöhung der Reaktivität. Die Reaktionszeit zur Herstellung von Atrazin wird beträchtlich reduziert.In addition to this fine particle size, the cyanuric chloride produced according to the invention surprisingly also already has a very high degree of purity (cyanuric chloride content> 99.5%, hydroxytriazines (0.5%, polytriazines <0.1%) and can therefore be processed directly in most cases without further cleaning operations With the cyanuric chloride according to the invention, for example, atrazine is obtained in a yield of 99%, which with cyanuric chloride obtained according to the prior art was not possible directly. The extremely high grain size also leads to a strong increase in reactivity. The reaction time for the production of atrazine is considerably reduced.
Das erfindungsgemäße Verfahren wird anhand der beigefügten Zeichnung und der Beispiele näher erläutert.The method according to the invention is explained in more detail with the aid of the attached drawing and the examples.
Die Zeichnung zeigt schematisch die erfindungsgemäße Gewinnung von festem Cyanurchlorid aus dem bei der Trimerisierung des Chlorcyans anfallenden Reaktionsgasgemisch. Der Cyanurchloriddampf wird durch Leitung (1) der Abscheidekammer (5) im unteren Teil zugeführt. Die Leitung (1) ist am Eintritt in die Kammer (5) schräg nach oben gerichtet. Durch die Düsen (2) wird Kaltluft eingeleitet. Nach der Desublimation wird der Feststoff über Leitung (3) ausgetragen, während die Abgase über die Leitung (4) am oberen Teil der Abscheidekammer (5) abgezogen werden.The drawing shows schematically the recovery of solid cyanuric chloride from the reaction gas mixture obtained during the trimerization of the cyanogen chloride. The cyanuric chloride vapor is fed through line (1) to the separation chamber (5) in the lower part. The line (1) is directed obliquely upwards at the entry into the chamber (5). Cold air is introduced through the nozzles (2). After desublimation, the solid is discharged via line (3), while the exhaust gases are drawn off via line (4) at the upper part of the separation chamber (5).
Nach dem Austritt aus dem Trimerisierungsreaktor wird der anfallende Cyanurchloriddampf, der noch Verunreinigungen wie z. B. Chlorcyan oder Chlor enthält, in einer Menge von 250 kg/h in den unteren Teil der Abscheidekammer (5) gemäß Zeichnung eingeleitet, wobei die Zuleitung (1) gegenüber der Horizontalen einen Winkel von 45° aufweist. Gleichzeitig leitet man 135 kg/h Kaltluft mit einer Temperatur von 25°C durch mehrere Düsen (2) in die Abscheidekammer (5) und bewirkt damit die Abscheidung des Cyanurchlorids. Während die Kaltluft zusammen mit den Restgasen am oberen Teil der Abscheidekammer abgezogen wird, fällt das feinteilige, feste Cyanurchlorid am Boden der Abscheidekammer an, wo es ausgetragen wird.After leaving the trimerization reactor, the resulting cyanuric chloride vapor, which still contains impurities such as e.g. B. contains chlorine or chlorine, in an amount of 250 kg / h in the lower part of the separation chamber (5) according to the drawing, the feed line (1) has an angle of 45 ° to the horizontal. At the same time, 135 kg / h of cold air at a temperature of 25 ° C are passed through several nozzles (2) into the separating chamber (5), thus causing the deposition of the cyanuric chloride. While the cold air is extracted together with the residual gases at the upper part of the separation chamber, the fine-particle, solid cyanuric chloride accumulates at the bottom of the separation chamber, where it is discharged.
Es weist folgende Kornverteilung auf:
Wie im Beispiel 1 beschrieben, werden 250 kg Cyanurchloriddampf stündlich in die Abscheidekammer zusammen mit 135 kg Kaltluft mit einer Temperatur von 10°C eingeleitet und abgeschieden.As described in Example 1, 250 kg of cyanuric chloride vapor are introduced into the separation chamber together with 135 kg of cold air at a temperature of 10 ° C. and separated off.
Das anfallende Cyanurchlorid besitzt folgende Kornverteilung:
Claims (6)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE3336993 | 1983-10-11 | ||
| DE19833336993 DE3336993A1 (en) | 1983-10-11 | 1983-10-11 | METHOD FOR PRODUCING SOLID CYANURCHLORIDE |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0141312A1 true EP0141312A1 (en) | 1985-05-15 |
| EP0141312B1 EP0141312B1 (en) | 1988-04-20 |
Family
ID=6211571
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP84112227A Expired EP0141312B1 (en) | 1983-10-11 | 1984-10-11 | Method for the preparation of solid cyanuric chloride |
Country Status (5)
| Country | Link |
|---|---|
| US (1) | US4535160A (en) |
| EP (1) | EP0141312B1 (en) |
| JP (1) | JPS6097965A (en) |
| DE (2) | DE3336993A1 (en) |
| ES (1) | ES8504154A1 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3514840A1 (en) * | 1985-04-24 | 1986-10-30 | Skw Trostberg Ag, 8223 Trostberg | METHOD FOR PRODUCING SOLID CYANURCHLORIDE |
| DE19642449A1 (en) | 1996-10-15 | 1998-04-16 | Degussa | Cyanuric chloride moldings and process for their manufacture |
| JP4839467B2 (en) * | 2008-05-13 | 2011-12-21 | 三井金属アクト株式会社 | Automotive door |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AT231995B (en) * | 1960-02-02 | 1964-02-25 | Lonza Ag | Process for purifying cyanuric chloride |
| DE2537673B1 (en) * | 1975-08-23 | 1977-02-17 | Degussa | Process for the production of finely divided, solid cyano chloride |
| DE2843379B2 (en) * | 1978-10-05 | 1980-07-10 | Deutsche Gold- Und Silber-Scheideanstalt Vormals Roessler, 6000 Frankfurt | Process for the recovery of solid cyanuric chloride |
| AT366378B (en) * | 1978-10-05 | 1982-04-13 | Degussa | METHOD FOR PRODUCING SOLID CYANURCHLORIDE |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2734058A (en) * | 1956-02-07 | Process for the production of solid finely | ||
| US2742977A (en) * | 1956-04-24 | Vapors of | ||
| US2753346A (en) * | 1956-07-03 | Huemer | ||
| GB1095454A (en) * | 1965-08-21 | |||
| US3539565A (en) * | 1968-01-29 | 1970-11-10 | Geigy Chem Corp | Method for producing a solution of cyanuric chloride from gaseous cyanuric chloride |
-
1983
- 1983-10-11 DE DE19833336993 patent/DE3336993A1/en not_active Withdrawn
-
1984
- 1984-07-31 US US06/636,335 patent/US4535160A/en not_active Expired - Lifetime
- 1984-08-03 ES ES534899A patent/ES8504154A1/en not_active Expired
- 1984-10-11 DE DE8484112227T patent/DE3470540D1/en not_active Expired
- 1984-10-11 EP EP84112227A patent/EP0141312B1/en not_active Expired
- 1984-10-11 JP JP59211598A patent/JPS6097965A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AT231995B (en) * | 1960-02-02 | 1964-02-25 | Lonza Ag | Process for purifying cyanuric chloride |
| DE2537673B1 (en) * | 1975-08-23 | 1977-02-17 | Degussa | Process for the production of finely divided, solid cyano chloride |
| DE2843379B2 (en) * | 1978-10-05 | 1980-07-10 | Deutsche Gold- Und Silber-Scheideanstalt Vormals Roessler, 6000 Frankfurt | Process for the recovery of solid cyanuric chloride |
| AT366378B (en) * | 1978-10-05 | 1982-04-13 | Degussa | METHOD FOR PRODUCING SOLID CYANURCHLORIDE |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6097965A (en) | 1985-05-31 |
| ES534899A0 (en) | 1985-04-16 |
| ES8504154A1 (en) | 1985-04-16 |
| DE3470540D1 (en) | 1988-05-26 |
| US4535160A (en) | 1985-08-13 |
| EP0141312B1 (en) | 1988-04-20 |
| DE3336993A1 (en) | 1985-04-25 |
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